JP2001296259A - X-ray diffraction apparatus - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an X-ray diffraction apparatus, having a structure capable of executing easily not only the post-evaluation of manufactured material but also the evaluation of the material during the manufacture, even in a corrosive reaction gas atmosphere in an MOCVD device (metall organic chemical vapor deposition device) which is hard measured by the conventional technology, connecting the X-ray diffracting device used for determination of a crystal structure of the material, evaluation of crystallinity or the like. SOLUTION: In this X-ray diffraction apparatus, having an X-ray diffracting chamber for investigating the structure of material through X-ray diffraction, at least a part where X-rays are transmitted of the X-ray diffracting chamber is manufactured from an X-ray transmission material, and corrosion resisting material with respect to the corrosive reaction gas is coated on the inner surface thereof, to thereby enable not only post-evaluation of the manufactured material but also evaluation of the material during the manufacture, in the presence of the reaction gas.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray diffractometer used for determining a crystal structure of a material, evaluating crystallinity, etc., and more particularly to an MOCVD apparatus (metal organic chemical vapor deposition apparatus).
And the like, the present invention relates to an X-ray diffraction apparatus having a structure capable of not only ex-post evaluation of a manufactured material but also evaluation of the material during the manufacturing even in the presence of a reactive gas.

[0002]

2. Description of the Related Art The X-ray diffraction method utilizes the law of Bragg reflection and is used to determine the crystal structure of a material, to evaluate crystallinity, and to evaluate semiconductor materials, metal materials, and polymer materials. It is an indispensable evaluation method. In particular, with the recent development of the material technology, not only ex-post evaluation of the produced material but also evaluation during the production of the material has been required. For this purpose, it is necessary to combine a material manufacturing apparatus and an X-ray diffraction apparatus, and various apparatuses have been devised.

FIG. 2 shows an example of a conventional X-ray diffractometer capable of measuring a material while heating it at a high temperature. The X-ray diffractometer is roughly composed of an X-ray goniometer 1 for performing a Bragg reflection measurement and an X-ray diffraction chamber 2 for holding a sample 4. The measurement of the X-ray diffraction is performed by using the X-ray provided on the side surface of the chamber 2.
The sample 4 set in the chamber 2 is irradiated with X-rays 5 through the radiation entrance window 3, and the Bragg reflection X
This is a method in which a line 6 is extracted and detected by a detector 8 through an X-ray extraction window 7.

[0004] This X-ray diffraction apparatus is, for example, an MOCVD apparatus (Metalorganic chemical 1 vapo) using a reactive gas.
r deposition: a metal organic chemical vapor deposition apparatus), there is a possibility that a reaction may occur with a material constituting the X-ray diffraction chamber 2 depending on a gas used. For example, when aluminum that easily transmits X-rays is used for a part of the chamber 2, TMG (Trimethygal) is used as a raw material gas.
When lium) is used, Ga atoms in TMG may react with aluminum and cause corrosion of the chamber 2 wall. In order to prevent this, if the chamber 2 is manufactured using quartz or a stainless steel plate which is usually used in an MOCVD apparatus, there arises a problem that X-rays are not transmitted, and it is difficult to perform X-ray diffraction. Becomes

Beryllium is usually used for the X-ray entrance window 3 or the X-ray extraction window 7 as shown in FIG. 2, but beryllium itself is not so strong and durable. In an atmosphere using an inert gas, an accident may occur due to cracks in the beryllium window or the like.

Furthermore, beryllium windows that can transmit X-rays while sealing the reaction gas are very expensive, and MOCVD to which the product of the reaction gas is liable to adhere.
It is not a suitable material for the device. A similar case occurs when, for example, a chlorine gas, a hydrogen sulfide gas, or the like is introduced into the chamber, and the initial corrosion process of the metal is examined.

[0007]

SUMMARY OF THE INVENTION An object of the present invention is to provide an X-ray diffractometer used for determining the crystal structure of a material, evaluating crystallinity, etc.
An X-ray diffractometer with a structure that can easily evaluate not only the ex-post evaluation of the manufactured material but also the material during the manufacturing even in a reactive gas atmosphere such as an OCVD apparatus (organic metal chemical vapor deposition apparatus). To provide.

[0008]

Means for Solving the Problems In order to solve the above-mentioned problems of the present invention, the present invention is configured as described in the claims. That is, as described in claim 1, an X-ray diffraction apparatus having an X-ray diffraction chamber for examining the structure of a substance by X-ray diffraction, wherein the X-ray diffraction chamber is at least one of the chambers through which X-rays pass. The wall part is made of X-ray permeable material, and the inner surface is coated with a substance that is resistant to corrosion by reactive gas. The X-ray diffraction apparatus is provided with an X-ray diffraction chamber having a structure capable of evaluating materials in the inside.

Further, as described in claim 2, claim 1
In the X-ray diffraction chamber of the X-ray diffraction apparatus according to the above,
An X-ray diffraction apparatus having a structure in which incident X-rays and Bragg-reflected X-rays pass through the wall of the chamber, which is partially detachable and can be attached.

[0010] Also, as described in claim 3, claim 1
Or in the X-ray diffraction chamber of the X-ray diffraction apparatus according to 2, wherein the material constituting the chamber is beryllium or an oxide of beryllium, a nitride, boron or an oxide of boron, a nitride, a carbide, a carbon or a carbide, Aluminum or an alloy containing aluminum as a main component, titanium or an alloy containing titanium as a main component, vanadium or an alloy containing vanadium as a main component, chromium or an alloy containing chromium as a main component, manganese or an alloy containing manganese as a main component An X-ray diffractometer made of at least one material selected from the above.

[0011] Also, as described in claim 4, claim 1
Or the X-ray diffraction chamber of the X-ray diffractometer according to 2, wherein the inner wall of the chamber is coated with at least one material selected from silicon oxide, carbon, beryllium, stainless steel, molybdenum, and monel alloy. X-ray diffractometer.

The X of the structure as described in the above-mentioned claims 1 to 4
By using an X-ray diffractometer equipped with a X-ray diffraction chamber, it can be manufactured even in a corrosive reaction gas atmosphere such as a MOCVD apparatus (metal organic chemical vapor deposition apparatus), which has been difficult to measure with the conventional technology. It is possible to easily evaluate not only the ex post facto evaluation of the material but also the material during fabrication.
It can greatly contribute to the development of semiconductor materials and metal materials.

In the X-ray diffractometer of the present invention, at least the X-ray entrance window and the X-ray extraction window are made of an X-ray transmissive material, and a corrosion-resistant substance against a reactive gas is formed on the inner surface. It has a coated X-ray diffraction chamber. When producing a material on a sample (for example, forming a film), the X-ray diffraction chamber heats the sample with a heater and introduces a reactive gas into the chamber through a gas inlet provided at an upper portion of the chamber. Is thermally decomposed on the sample to form a film. The gas after the reaction is exhausted from the exhaust port to the outside of the chamber, and is detoxified by the abatement apparatus. By taking such a process, it becomes possible to produce a material on a sample, to perform X-ray diffraction at each stage of the process, to determine the crystal structure of the material, to evaluate the crystallinity, etc. It can contribute to the development of semiconductor materials, metal materials, and the like.

The material of the X-ray diffraction chamber of the present invention may be, for example, beryllium or beryllium oxide or nitride.
Boron or oxides of boron, nitrides, carbides, etc., carbon or carbides, aluminum or aluminum-based alloys, titanium or titanium-based alloys, vanadium or vanadium-based alloys, chromium or One or more of chromium-based alloys, manganese, and manganese-based alloys can be arbitrarily selected and used.

As the corrosion-resistant coating material on the inner surface of the X-ray diffraction chamber, at least one selected from silicon oxide, carbon, beryllium, stainless steel, molybdenum or monel alloy can be arbitrarily selected and used. As long as it has good corrosion resistance to the reactive gas, its type is not particularly specified.

[0016]

FIG. 2 shows an example of the configuration of an X-ray diffraction apparatus according to the present invention. Hereinafter, embodiments of the present invention will be described, but the present invention is not limited to these embodiments. <Embodiment> Using an X-ray diffractometer equipped with an X-ray diffraction chamber shown in FIG. 1, a GaAs crystal is produced using TMG (trimethylgallium) and arsine (AsH ₃ ) as a reactive gas. Its crystallinity can be evaluated by X-ray diffraction. FIG. 1 is a schematic diagram showing the configuration of the entire X-ray diffraction apparatus used in the present embodiment. The X-ray diffraction measurement part of this device is a conventional X-ray diffraction device shown in FIG.
The structure is almost the same as that of the X-ray diffraction apparatus, but the structure of the X-ray diffraction chamber for setting a sample is different. X
In order to perform X-ray diffraction, a sample 11 set in an X-ray diffraction chamber (also a reaction chamber) 10 is irradiated with incident X-rays 9,
A Bragg reflected X-ray 12 generated by the sample 11 is measured by a detector 13. Here, X-ray diffraction chamber 1
As shown in FIG. 1B, reference numeral 0 denotes a chamber outer wall 15 that easily transmits X-rays and a coating layer 16 that does not react with TMG.

In order to prepare a material on the sample 11, the sample 11 is heated by a heater 14, and a reactive gas 17 is supplied from a gas inlet 18 provided in the upper part of the X-ray diffraction chamber 10 to the chamber. 10 and thermally decomposed on the sample 11. The gas after the reaction that has passed over the sample 11 is exhausted from the exhaust port 19 to the outside of the chamber 10, and is detoxified by the abatement apparatus. By performing such a process, it is possible to produce a material on the sample 11.

A problem in performing X-ray diffraction using the X-ray diffraction apparatus of the present invention is the absorptivity of X-rays by the X-ray diffraction chamber 10. When an aluminum plate having a thickness of about 2 mm is used as an outer wall of the chamber 10 and X-rays having a wavelength of 0.06 nm are used, about 30% of the X-rays are absorbed by the outer wall of the chamber 10. The inner wall of the chamber 10 is coated with silicon oxide that does not react with TMG to a thickness of about 0.1 μm, and the X-ray absorption here is 1% or less, which is almost negligible. Therefore, the total absorptivity of the X-rays was about 30%, and it was found that the measurement accuracy and time were not significantly affected.

As described above in the present embodiment, in the X-ray diffraction apparatus provided with the X-ray diffraction chamber of the present invention,
Material preparation process and X-ray measurement can be performed simultaneously,
X-ray diffraction measurement during material production becomes possible.

In this embodiment, aluminum is used as a material for forming the X-ray diffraction chamber, and silicon oxide is used as a material for coating the inner wall of the chamber. Materials such as beryllium or beryllium oxides and nitrides, boron or boron oxides, nitrides, carbides, etc., carbon or carbides, etc., alloys mainly composed of aluminum, titanium or alloys mainly composed of titanium , Vanadium or an alloy containing vanadium as a main component, chromium or an alloy containing chromium as a main component, manganese or an alloy containing manganese as a main component, and the use of at least one of them is confirmed. In addition, it has been confirmed that at least one selected from arbitrarily selected from silicon oxide, carbon, beryllium, stainless steel, molybdenum, monel alloy and the like is used as a coating material for the inner surface of the chamber.

[0021]

According to the present invention, an X-ray provided with an X-ray diffraction chamber according to the present invention.
By using the X-ray diffraction apparatus, it is possible to easily use X-ray diffraction for evaluating materials in a reactive gas or a corrosive gas, and to contribute to the development of semiconductor materials and metal materials.

[Brief description of the drawings]

FIG. 1 is a schematic diagram showing a structure of an X-ray diffraction apparatus having an X-ray diffraction chamber exemplified in an embodiment of the present invention.

FIG. 2 is a schematic view showing the structure of a conventional X-ray diffraction apparatus.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 ... X-ray goniometer 2 ... X-ray diffraction chamber 3 ... X-ray incidence window 4 ... Sample 5 ... Incident X-ray 6 ... Bragg reflection X-ray 7 ... X-ray extraction window 8 ... Detector 9 ... Incident X-ray REFERENCE SIGNS LIST 10 X-ray diffraction chamber (also reaction chamber) 11 Sample 12 Bragg reflection X-ray 13 Detector 14 Heater 15 Chamber outer wall 16 Coating layer 17 Reactive gas 18 Gas inlet 19 Exhaust port 20 ... X-ray incidence part 21 ... X-ray extraction part

 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 2G001 AA01 BA18 CA01 GA01 GA13 JA08 JA14 KA08 LA02 NA03 NA06 NA07 NA10 NA17 PA07 QA02 QA03 QA10 RA03 RA08 SA16 4K030 AA05 AA11 BA08 BA25 FA10 KA41

Claims (4)

[Claims] 1. An X-ray diffractometer having an X-ray diffraction chamber for examining the structure of a substance by X-ray diffraction,
In the X-ray diffraction chamber, at least a wall portion of the chamber through which X-rays are transmitted is made of an X-ray permeable material, and an inner surface thereof is coated with a substance which is resistant to a reactive gas, so that the presence of the reactive gas is prevented. An X-ray diffraction chamber having a structure capable of not only ex-post evaluation of the manufactured material but also evaluation of the material during the manufacturing is provided below.
Line diffractometer. 2. An X-ray diffraction chamber of an X-ray diffraction apparatus according to claim 1, wherein a wall portion of said chamber through which incident X-rays and Bragg-reflected X-rays can be partially removed and attached. An X-ray diffraction apparatus, characterized in that: 3. An X-ray diffraction chamber of an X-ray diffraction apparatus according to claim 1, wherein the material constituting the chamber is beryllium, beryllium oxide, nitride, boron or boron oxide, nitride. Material, carbide, carbon or carbide, aluminum or an alloy mainly containing aluminum, titanium or an alloy mainly containing titanium, vanadium or an alloy mainly containing vanadium, chromium or an alloy mainly containing chromium, manganese or An X-ray diffraction apparatus comprising at least one material selected from alloys containing manganese as a main component. 4. The X-ray diffraction chamber of an X-ray diffraction apparatus according to claim 1, wherein an inner wall of the chamber is
An X-ray diffractometer characterized by being coated with at least one material selected from silicon oxide, carbon, beryllium, stainless steel, molybdenum, and monel alloy.